CN111530634A - Flotation method of alkaline granite type rare earth ore - Google Patents
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
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- B03D1/001—Flotation agents
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- B03D1/014—Organic compounds containing phosphorus
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
- B03D1/025—Froth-flotation processes adapted for the flotation of fines
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
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Abstract
The invention provides a flotation method of alkaline granite rare earth ore. According to the types and characteristics of rare earth minerals in ores, the flotation process flow and parameters suitable for alkaline granite rare earth minerals are invented, three collectors of oxidized kerosene, benzohydroxamic acid and tributyl phosphate are used in a combined mode, and are cooperated with each other in the process of flotation of the rare earth minerals, so that efficient flotation of the rare earth minerals is achieved, the recovery rate and the grade of the rare earth during flotation of the alkaline granite rare earth minerals are improved, the yield of the rare earth concentrate is 3.87%, the grade of the rare earth concentrate is 12.87%, and the recovery rate is 78.73%.
Description
Technical Field
The invention belongs to the technical field of mineral separation, and particularly relates to a flotation method of alkaline granite type rare earth ore.
Background
The rare earth element has excellent chemical and physical properties, so that the rare earth element is widely applied to the industries of metallurgy, chemical engineering, petroleum, electronics, medicine, agriculture and the like, and particularly plays an important role in the high-tech field, such as permanent magnetic materials, magneto-optical storage materials, magnetostrictive materials, luminescent materials and catalytic materials. China is a big rare earth country in the world, not only has abundant reserves, but also has the advantages of complete ore species and rare earth elements, reasonable distribution of rare earth grade high-grade ore points and the like, and lays a solid foundation for the development of the rare earth industry in China.
The Bazhen rare earth ore in great Xingan mountain of inner Mongolia of China belongs to alkaline granite type rare earth ore deposit, and is ultra-large rare earth metal ore. The main rare earth minerals are silicon beryllium yttrium cerium ore, black rare gold and monazite, and then the easy-to-dissolve stone, cerium-uranium ilmenite and the like, wherein the silicon beryllium yttrium cerium ore is a new mineral of rare earth and beryllium with industrial value found in granite type rare metal ores in the end of the 70 th 20 th century. The silicon-beryllium-yttrium-cerium ore has the advantages of multiple mineral composition elements, complex chemical structure, various mineral surface properties, multiple factors influencing floatability and high difficulty in flotation separation and enrichment, and belongs to the class of minerals difficult to float. The Bazhen minerals have complex composition, more rare earth minerals, low grade and great difficulty in the dressing and metallurgy technology, and mineral dressing products with high recovery rate and high enrichment ratio are difficult to obtain, so that the economic development of the deposit is restricted.
Disclosure of Invention
The invention mainly aims to provide a flotation method of alkaline granite rare earth ore, which improves the recovery rate and grade of rare earth during flotation of the alkaline granite rare earth ore.
The technical scheme adopted by the invention is as follows:
a flotation method of alkaline granite type rare earth ore comprises the following steps:
(1) crushing and grinding ores: after the ore is crushed to-2 mm, the fineness is ground to-0.038 mm, which accounts for 40-90%.
(2) Preparing flotation pulp: and (3) putting the prepared ore pulp into a flotation machine, and adjusting the concentration of the ore pulp to be 10-35% and the temperature of the ore pulp to be 30-80 ℃.
(3) Adjusting ore pulp: adding 200-2000 g/t of sodium carbonate into the ore pulp, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 0-3000 g/t of water glass and 0-1000 g/t of carboxymethyl cellulose, stirring at a speed of 500-2500 r/min, and stirring for 3-15 min; adding 200-1500g/t of sodium fluosilicate, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min.
(4) Flotation of rare earth minerals: adding 1500g/t of collecting agent oxidized kerosene 200-; adding 50-300g/t of auxiliary collecting agent tributyl phosphate, stirring at the speed of 500-2500 r/min for 3-15 min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings;
(5) adding 50-300g/t of collecting agent oxidized kerosene and 50-200g/t of benzohydroxamic acid into the roughed tailings obtained in the step (4), stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 30-200 g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 500-2500 r/min for 3-15 min, and scavenging for 1-2 times to obtain scavenged concentrate and flotation tailings;
(6) and (4) merging the roughing concentrates obtained in the step (4) and the scavenging concentrates obtained in the step (5), carrying out concentration for multiple times, and returning the concentrated tailings to the previous flotation stage until the ideal flotation index is reached.
Wherein, the fineness in the step (1) is ground to-0.038 mm, which accounts for 90 percent.
The sodium carbonate added in the step (3) is 1200g/t, and the stirring time is 5 min; the added water glass is 1000g/t, the added carboxymethyl cellulose is 200g/t, and the stirring time is 5 min.
The oxidized kerosene added in the step (4) is 800g/t, the benzohydroxamic acid is 200g/t, and the stirring time is 5 min.
The tributyl acid ester added in the step (4) is 150g/t, and the stirring time is 5 min.
150g/t of oxidized kerosene and 50g/t of benzohydroxamic acid are added in the step (5), and the stirring time is 5 min.
The tributyl acid ester added in the step (5) is 50g/t, and the stirring time is 5 min.
The invention provides a flotation method of alkaline granite rare earth ore. According to the types and characteristics of rare earth minerals in ores, the flotation process flow and parameters suitable for alkaline granite rare earth ores are invented, three collectors of oxidized kerosene, benzohydroxamic acid and tributyl phosphate are used in a combined mode, and are cooperated with each other in the rare earth mineral flotation process, so that efficient flotation of the rare earth minerals is achieved, the yield of the rare earth concentrate is 3.87%, the grade is 12.87%, and the recovery rate is 78.73%. Effectively solves the problems of low rare earth recovery rate and low grade in the flotation of the alkaline granite rare earth ore at present.
Drawings
FIG. 1 is a schematic diagram of a flotation process for alkaline granite rare earth ore.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
As shown in fig. 1, the present invention provides a flotation method of alkaline granite type rare earth ore, comprising the steps of:
(1) crushing and grinding ores: after the ore is crushed to-2 mm, the fineness is ground to-0.038 mm, which accounts for 40-90%.
(2) Preparing flotation pulp: and (3) putting the prepared ore pulp into a flotation machine, and adjusting the concentration of the ore pulp to be 10-35% and the temperature of the ore pulp to be 30-80 ℃.
(3) Adjusting ore pulp: adding 200-2000 g/t of sodium carbonate into the ore pulp, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 0-3000 g/t of water glass and 0-1000 g/t of carboxymethyl cellulose, stirring at a speed of 500-2500 r/min, and stirring for 3-15 min; adding 200-1500g/t of sodium fluosilicate, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min.
(4) Flotation of rare earth minerals: adding 1500g/t of collecting agent oxidized kerosene 200-; adding 50-300g/t of auxiliary collecting agent tributyl phosphate, stirring at the speed of 500-2500 r/min for 3-15 min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings;
(5) adding 50-300g/t of collecting agent oxidized kerosene and 50-200g/t of benzohydroxamic acid into the roughed tailings obtained in the step (4), stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 30-200 g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 500-2500 r/min for 3-15 min, and scavenging for 1-2 times to obtain scavenged concentrate and flotation tailings;
(6) and (4) merging the roughing concentrates obtained in the step (4) and the scavenging concentrates obtained in the step (5), carrying out concentration for multiple times, and returning the concentrated tailings to the previous flotation stage until the ideal flotation index is reached.
Wherein, the fineness in the step (1) is ground to-0.038 mm, which accounts for 90 percent.
The sodium carbonate added in the step (3) is 1200g/t, and the stirring time is 5 min; the added water glass is 1000g/t, the added carboxymethyl cellulose is 200g/t, and the stirring time is 5 min.
The oxidized kerosene added in the step (4) is 800g/t, the benzohydroxamic acid is 200g/t, and the stirring time is 5 min.
The tributyl acid ester added in the step (4) is 150g/t, and the stirring time is 5 min.
150g/t of oxidized kerosene and 50g/t of benzohydroxamic acid are added in the step (5), and the stirring time is 5 min.
The tributyl acid ester added in the step (5) is 50g/t, and the stirring time is 5 min.
The invention provides a flotation method of alkaline granite rare earth ore. According to the types and characteristics of rare earth minerals in ores, the flotation process flow and parameters suitable for alkaline granite rare earth ores are invented, three collectors of oxidized kerosene, benzohydroxamic acid and tributyl phosphate are used in a combined mode, and are cooperated with each other in the rare earth mineral flotation process, so that efficient flotation of the rare earth minerals is achieved, the yield of the rare earth concentrate is 3.87%, the grade is 12.87%, and the recovery rate is 78.73%. Effectively solves the problems of low rare earth recovery rate and low grade in the flotation of the alkaline granite rare earth ore at present.
Example 1
The main useful minerals in the barre's philosophy rare earth ore are hydroxylsilite-yttrium-cerium ore, niobite, zircon, zinc solar garnet, pyrochlore, monazite and the like, the gangue minerals are quartz, potassium feldspar, albite, amphibole, calcite and the like, and the REO content in the ore is 0.63 percent.
(1) Firstly, crushing ore to-2 mm, then grinding the crushed ore to 50% of-0.038 mm, adjusting the concentration of ore pulp to 25%, adjusting the temperature of the ore pulp to 35 ℃, and putting the ore pulp into a flotation tank.
(2) Adding 500g/t of sodium carbonate into the ore pulp, stirring at the speed of 1500r/min for 5 min; adding 800g/t of water glass and 200g/t of carboxymethyl cellulose, stirring at the speed of 1500r/min, and stirring for 5 min; adding 500g/t of sodium fluosilicate, stirring at the speed of 1500r/min, and stirring for 5 min.
(3) Adding 400g/t of collecting agent oxidized kerosene and 300g/t of benzohydroxamic acid into the ore pulp, stirring at the speed of 1500r/min for 5 min; and adding 100g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 1500r/min for 5min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings.
(4) Adding 100g/t of oxidized kerosene and 100g/t of benzohydroxamic acid into the roughed tailings, stirring at the speed of 1500r/min for 5 min; and adding 50g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 1500r/min for 5min, scavenging for 1 time to obtain scavenged concentrate and flotation tailings, and concentrating the roughed concentrate for three times to obtain rare earth concentrate. Example 1 the results of the test are shown in table 1.
Table 1 example 1 test results
| Mineral processing product | Yield/%) | REO grade/% | Percent recovery% |
| Rougher concentrate | 2.63 | 11.78 | 49.09 |
| Scavenging concentrates | 8.61 | 0.49 | 6.68 |
| Middling 3 | 5.23 | 2.72 | 22.54 |
| Middling 2 | 5.14 | 0.67 | 5.46 |
| Middling 1 | 16.25 | 0.21 | 5.41 |
| Flotation of tailings | 62.14 | 0.11 | 10.83 |
| Raw ore | 100.00 | 0.63 | 100.00 |
Example 2
The main useful minerals in the barre's philosophy rare earth ore are hydroxylsilite-yttrium-cerium ore, niobite, zircon, zinc solar garnet, pyrochlore, monazite and the like, the gangue minerals are quartz, potassium feldspar, albite, amphibole, calcite and the like, and the REO content in the ore is 0.63 percent.
(1) Firstly, crushing ore to-2 mm, then grinding the crushed ore to 70% of-0.038 mm, adjusting the concentration of ore pulp to 30%, adjusting the temperature of the ore pulp to 45 ℃, and putting the ore pulp into a flotation tank.
(2) Adding 1000g/t of sodium carbonate into the ore pulp, stirring at 2000r/min for 10 min; adding 900g/t of water glass and 300g/t of carboxymethyl cellulose, stirring at the speed of 2000r/min for 10 min; 600g/t of sodium fluosilicate is added, the stirring speed is 2000r/min, and the stirring is carried out for 10 min.
(3) Adding 500g/t of collecting agent oxidized kerosene and 200g/t of benzohydroxamic acid into the ore pulp, stirring at the speed of 2000r/min for 10 min; adding 80g/t of auxiliary collecting agent tributyl phosphate, stirring at the speed of 2000r/min for 10min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings.
(4) Adding 200g/t of oxidized kerosene and 50g/t of benzohydroxamic acid into the roughed tailings, stirring at the speed of 2000r/min for 10 min; and adding 50g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 2000r/min for 10min, scavenging for 1 time to obtain scavenged concentrate and flotation tailings, and concentrating the roughed concentrate for 4 times to obtain rare earth concentrate. Example 2 the test results are shown in table 2.
Table 2 example 2 test results
| Mineral processing product | Yield/%) | REO grade/% | Percent recovery% |
| Rougher concentrate | 2.43 | 13.12 | 49.97 |
| Scavenging concentrates | 8.46 | 0.32 | 4.24 |
| Middling 4 | 3.24 | 2.14 | 10.87 |
| Middling 3 | 4.21 | 0.58 | 14.12 |
| Middling 2 | 5.98 | 0.32 | 5.44 |
| Middling 1 | 14.78 | 0.21 | 4.86 |
| Flotation of tailings | 60.90 | 0.11 | 10.50 |
| Raw ore | 100.00 | 0.64 | 100.00 |
Example 3
The main useful minerals in the barre's philosophy rare earth ore are hydroxylsilite-yttrium-cerium ore, niobite, zircon, zinc solar garnet, pyrochlore, monazite and the like, the gangue minerals are quartz, potassium feldspar, albite, amphibole, calcite and the like, and the REO content in the ore is 0.63 percent.
(1) Firstly, crushing ore to-2 mm, then grinding the crushed ore until the granularity of-0.038 mm accounts for 80%, adjusting the concentration of ore pulp to 30%, adjusting the temperature of the ore pulp to 45 ℃, and putting the ore pulp into a flotation tank.
(2) Adding 1200g/t of sodium carbonate into the ore pulp, stirring at the speed of 2000r/min for 5 min; adding 1000g/t of water glass and 200g/t of carboxymethyl cellulose, stirring at the speed of 2000r/min for 5 min; adding 600g/t of sodium fluosilicate, stirring at the speed of 2000r/min, and stirring for 5 min.
(3) Adding 800g/t of collecting agent oxidized kerosene and 200g/t of benzohydroxamic acid into the ore pulp, stirring at the speed of 2000r/min for 5 min; and adding 150g/t of auxiliary collecting agent tributyl phosphate, stirring at the speed of 2000r/min for 5min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings.
(4) 150g/t of oxidized kerosene and 50g/t of benzohydroxamic acid are added into the roughed tailings, the stirring speed is 2000r/min, and the stirring time is 5 min; and adding 100g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 2000r/min for 5min, and scavenging the rougher tailings for 1 time to obtain scavenged concentrate and flotation tailings.
(5) And combining the roughing concentrate and the scavenging concentrate, then carrying out concentration for 4 times, and returning the concentrated tailings to the previous stage for flotation in sequence to obtain the rare earth concentrate. The results are shown in Table 3.
Table 3 example 3 closed loop test results
| Mineral processing product | Yield/%) | REO grade/% | Percent recovery% |
| Rare earth concentrate | 3.87 | 12.87 | 78.73 |
| Flotation of tailings | 96.13 | 0.14 | 21.27 |
| Raw ore | 100.00 | 0.63 | 100.00 |
Claims (8)
1. A flotation method of alkaline granite type rare earth ore is characterized in that: the method comprises the following steps:
(1) crushing and grinding ores: crushing the ore to-2 mm, and grinding the ore to-0.038 mm, wherein the fineness of the ore is 40-90%;
(2) preparing flotation pulp: putting the prepared ore pulp into a flotation machine, and adjusting the concentration of the ore pulp to be 10-35% and the temperature of the ore pulp to be 30-80 ℃;
(3) adjusting ore pulp: adding 200-2000 g/t of sodium carbonate into the ore pulp, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 0-3000 g/t of water glass and 0-1000 g/t of carboxymethyl cellulose, stirring at a speed of 500-2500 r/min, and stirring for 3-15 min; adding 200-1500g/t of sodium fluosilicate, stirring at the speed of 500-2500 r/min, and stirring for 3-15 min;
(4) flotation of rare earth minerals: adding 1500g/t of collecting agent oxidized kerosene 200-; adding 50-300g/t of auxiliary collecting agent tributyl phosphate, stirring at the speed of 500-2500 r/min for 3-15 min, and performing air flotation after the collecting agent and the rare earth minerals fully act to obtain roughed concentrate and roughed tailings;
(5) adding 50-300g/t of collecting agent oxidized kerosene and 50-200g/t of benzohydroxamic acid into the roughed tailings obtained in the step (4), stirring at the speed of 500-2500 r/min, and stirring for 3-15 min; adding 30-200 g/t of tributyl phosphate serving as an auxiliary collecting agent, stirring at the speed of 500-2500 r/min for 3-15 min, and scavenging for 1-2 times to obtain scavenged concentrate and flotation tailings;
(6) and (4) merging the roughing concentrates obtained in the step (4) and the scavenging concentrates obtained in the step (5), carrying out concentration for multiple times, and returning the concentrated tailings to the previous flotation stage until the ideal flotation index is reached.
2. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the fineness in the step (1) is ground to-0.038 mm, and the ground fineness accounts for 90%.
3. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the amount of the sodium carbonate added in the step (3) is 1200g/t, and the stirring time is 5 min.
4. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the amount of the water glass added in the step (3) is 1000g/t, the amount of the carboxymethyl cellulose is 200g/t, and the stirring time is 5 min.
5. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the amount of the oxidized kerosene added in the step (4) is 800g/t, the amount of the benzohydroxamic acid is 200g/t, and the stirring time is 5 min.
6. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the tributyl acid ester added in the step (4) is 150g/t, and the stirring time is 5 min.
7. The flotation process for alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: 150g/t of oxidized kerosene, 50g/t of benzohydroxamic acid and 5min of stirring are added in the step (5).
8. The method for the flotation of alkaline granite-type rare-earth ores as claimed in claim 1, characterized in that: the tributyl acid ester added in the step (5) is 50g/t, and the stirring time is 5 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112337641A (en) * | 2020-09-01 | 2021-02-09 | 核工业北京化工冶金研究院 | Method for selecting niobium concentrate from polymetallic ore containing rare earth, niobium, zirconium and the like |
| CN113731627A (en) * | 2021-09-06 | 2021-12-03 | 核工业北京化工冶金研究院 | Pre-tailing-discarding mixed flotation method for rare earth multi-metal ore |
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